反应详情

温度

50 °C

To a suspension of 60% sodium hydride (8.24 g) in DMF (200 ml) was added dropwise dimethyl malonate (24.9 g) under ice-cooling, and the suspension was stirred at 50° C. for 30 min. After cooling to room temperature, a solution of 2-(2-fluorophenyl)ethyl methanesulfonate in DMF (30 ml) was added dropwise, and the mixture was stirred at 150° C. for 1 hr. After cooling to room temperature, the reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure to give dimethyl 2-[2-(2-fluorophenyl)ethyl]malonate.

1. temperaturecooling
2. temperatureAfter cooling to room temperature
3. stirringthe mixture was stirred at 150° C. for 1 hr
4. temperatureAfter cooling to room temperature
5. extractionthe mixture was extracted with ethyl acetate
6. washThe extract was washed with water and saturated brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure